Process of polymerizing butadiene hydrocarbons in the emulsified state



Patented Mar. 29, 1932 UNITED STATES PATENT OFFICE HANS LECHER, OF LEVERKUSEN/RHIITIE, AND ALBERT KOCH, OF OOLOGNE-DEUTZ, GERMANY, ASSIGNORS TO I. G, FARBENINDUSTRIE AKTIENGESELLSCHAFT, OF FRANKFOIRT-ON-THE-MAIN, GERMANY, A CORPORATION OF GERMANY PROCESS OF IOLYMERIZING BUTADIEN E HYDROCARBONS IN THE EMULSIFIED STATE No Drawing. Application filed March 7, 1929, Serial No. 345,219, and in Germany March 1' 7, 192%.

' The present invention relates to a process of polymerizing butadiene hydrocarbons in ring these emulsions at normal or slightly p elevated temperatures.

We have found, that the manufacture of butadiene hydrocarbons in water is facilitated and the stability of the emulsions is raised, when preparing thesame in the presence of both a water soluble emulsifying agent and an emulsifying agent which is soluble in the hydrocarbon to be polymerized. As Water soluble emulsifying agents may be mentioned by way of example'soaps, alkali metal salts of bile .acids, water soluble salts of thus obtained yielding a rubber like coagulate alkylated naphthalene sulfonic acids and the like. Butadiene hydrocarbon soluble emulsifying agentsare, for example, aluminumor alkali earth metal salts of palmitic acid, oleic acid, stearic acid or other higher fatty acids, etc.

An aqueous solution of a water soluble emulsifying agent emulsifies the butadiene hydrocarbon, yielding an emulsion with the hydrocarbon in dispersed phase. A solutidn pending on the quantities of the particular of an emulsifying agent which is soluble in a butadiene hydrocarbon emulsifies water,

. whereby an emulsion with water in dispersed phase is formed. Now, when emulsifying the aqueous solution of the water soluble emulsifying agent with that of the butadiene hydrocarbon soluble emulsifying agent in a butadiene hydrocarb n, there are easily formed stable emulsions with the water or the hydrocarbon" as the dispersed phase deemulsifying agents used. If desired, our emulsion may be homogenizedbefore polymerization in any desired manner, for example, by forcing them through small apertures.

The emulsions thus obtainable yield polymerization products according to the usual the hydrotiii- .in a closed vessel.

or elevated temperature, in a good yield con- I siderably surmounting in many cases, especially when the hydrocarbon is in dispersed phase, the yield which' is obtainable according to the methods hitherto known. .A further advantage of ournew process is, that worthless 4 by-products, such as terpene-like compounds are not formed either during the emulsifying or during the polymerization rocess. v

The following examples illustrate our invention, without limiting it thereto, the parts being by weight:

Ewample 1.7 5 parts, of an aqueous solution of sodium oleate of 10% strength and a solution of 2.5 parts of magnesium oleate in 50'parts of butadiene- (1.3; are caused to mixture in a closed vessel. Polymerization is then-performed by heating the emulsion to form an emulsion by shaking or stirring the C. for about 6 days. A latexlike mass is I for example, by acidifying, inan excellent yield. By vulcanizing this coagulate a prodplacing the butadiene-(L3) by 50 parts'of isoprene.

Example 2.100 parts of an aqueous solution of sodium stearate of 7% strength are emulsified with parts of 2.3-dimethylbutadiene-(1.3') containing in solution 3 parts of magnesium oleate by stirring the mixture Polymerization is then performed by heating the emulsion to 70 C.

for about 5 days, while continually shaking.

A latex like cream is'thus obtained in a nearly quantitative yield, yielding a rubber like mass by coagulation and Washing.

Ewam Ze-8.1OO parts of an aqueous sodium oleate solution of 10% strength are excellent yield b freezing out and washing. Example 4. mixture of parts of an aqueous sodium oleate solution of 10% strength, 5 parts of normal caustiosoda solution, parts of magnesium oleate and 60 parts of butadiene- (1.3) is emulsified by shaking in a closed vessel. The emulsion thus formed is homogenized in a homogenizer of any desired kind and then polymerized by heating to about 60 C. for about- 3 days without shaking or stirring. A quantitative yield of a latex like mass is thus obtained yielding a coagulate by freezing out.

In all the examples the yields of polymerization products are considerably better than the yields obtainable according to the same.

methods but without the addition of a butadiene hydrocarbon soluble emulsifyingagent.

We claim 1. A process which comprises emulsifying a butadiene hydrocarbon in water in the presence of both an emulsifying agent which is soluble in water and an emulsifying agent which is soluble in the butadiene hydrocarbon and then polymerizing the butadiene hydrocarbon.

2. A process which comprises emulsifying a compound of the group consisting of hutadiene-(1.3), isoprene and 2.3-dimethylbutadiene- (1.3) in water in the presence of both an emulsifying agent which is soluble in water and an emulsifying agent which is soluble in the said compound and then merizing said compound.

3. A process which comprises emulsifying a butadiene hydrocarbon in water in the presence of both an emulsifying agent which is soluble in water and an emulsifying-agent which is soluble in the butadiene hydrocarbon,'homogenizi ng the emulsion and then polymerizing the butadiene hydrocarbon.

4. A process which comprises emulsifying a compound of the group consisting of hutadiene-(1.3), isoprene and 2.3-dimethylbutadiene- 1.3) in water in the presence of both an emulsifying agent which is soluble in water and an emulsifying agent which is soluble in the said compound, homogenizing the emulsion and then polymerizing the butadiene hydrocarbon. V

In testimony whereof we have hereunto set our hands. H HANS LECHER. [11. s.] ALBERT KOCH. [L.s.]

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